印染助剂
印染助劑
인염조제
TEXTILE AUXILIARIES
2014年
8期
50-52
,共3页
任忠海%李天宝%刘庆备%叶林
任忠海%李天寶%劉慶備%葉林
임충해%리천보%류경비%협림
N-甲基吡咯烷酮%气相色谱-质谱法%芳纶纤维%溶剂残留物
N-甲基吡咯烷酮%氣相色譜-質譜法%芳綸纖維%溶劑殘留物
N-갑기필각완동%기상색보-질보법%방륜섬유%용제잔류물
N-methylpyrrolidinone (NMP)%GC/MS%aramid fiber%solvent residues
芳纶纤维在合成过程中常使用N-甲基吡咯烷酮作为反应溶剂,通过对提取方法和色谱、质谱条件的改进,建立了芳纶纤维中溶剂残留物N-甲基吡咯烷酮(NMP)的气相色谱-质谱联用(GC/MS)测定法.芳纶纤维试样经乙酸乙酯超声波提取,提取液浓缩后用滤纸过滤,用气相色谱-质谱仪测定,外标法定量,选择离子监测进行阳性确证.结果表明,当添加N-甲基吡咯烷酮1~10μg/mL时,待测芳纶纤维试样中N-甲基吡咯烷酮的回收率达95.8%,相对标准偏差RSD(n=7)小于5%,其最低检出限为0.05μg/mL.本方法操作简单、灵敏度高、重现性好,可用于芳纶纤维中N-甲基吡咯烷酮残留量分析.
芳綸纖維在閤成過程中常使用N-甲基吡咯烷酮作為反應溶劑,通過對提取方法和色譜、質譜條件的改進,建立瞭芳綸纖維中溶劑殘留物N-甲基吡咯烷酮(NMP)的氣相色譜-質譜聯用(GC/MS)測定法.芳綸纖維試樣經乙痠乙酯超聲波提取,提取液濃縮後用濾紙過濾,用氣相色譜-質譜儀測定,外標法定量,選擇離子鑑測進行暘性確證.結果錶明,噹添加N-甲基吡咯烷酮1~10μg/mL時,待測芳綸纖維試樣中N-甲基吡咯烷酮的迴收率達95.8%,相對標準偏差RSD(n=7)小于5%,其最低檢齣限為0.05μg/mL.本方法操作簡單、靈敏度高、重現性好,可用于芳綸纖維中N-甲基吡咯烷酮殘留量分析.
방륜섬유재합성과정중상사용N-갑기필각완동작위반응용제,통과대제취방법화색보、질보조건적개진,건립료방륜섬유중용제잔류물N-갑기필각완동(NMP)적기상색보-질보련용(GC/MS)측정법.방륜섬유시양경을산을지초성파제취,제취액농축후용려지과려,용기상색보-질보의측정,외표법정량,선택리자감측진행양성학증.결과표명,당첨가N-갑기필각완동1~10μg/mL시,대측방륜섬유시양중N-갑기필각완동적회수솔체95.8%,상대표준편차RSD(n=7)소우5%,기최저검출한위0.05μg/mL.본방법조작간단、령민도고、중현성호,가용우방륜섬유중N-갑기필각완동잔류량분석.
N-methylpyrrolidinone (NMP) was commonly used as reaction solvents in the synthesis of ara-mid fiber. A gas chromatography/mass spectrometry (GC/MS) method of determination of N-methylpyrrolidi-none in textiles was established by improving the extraction method and GC/MS conditions. The samples were extracted with ethyl acetate by ultrasound assisted procedure.After being concentrated and purified with filter paper, the extract was quantitatively determined using GC/MS by external standard method and positive-ly confirmed through selected-ion monitoring mode. The results showed that while the dosage of N-methyl-pyrrolidinone was 1~10 μg/mL, the method provided 95.8% of recovery rate, lower than 5% of relative stan-dard deviations and 0.05 μg/mL of determination limit. The method was simple, and had high sensitivity and good repeatability, which could be used in the residual content determination of NMP in aramid fiber.